CN201075087Y - Device for analyzing quicksilver element form - Google Patents
Device for analyzing quicksilver element form Download PDFInfo
- Publication number
- CN201075087Y CN201075087Y CNU2007201700393U CN200720170039U CN201075087Y CN 201075087 Y CN201075087 Y CN 201075087Y CN U2007201700393 U CNU2007201700393 U CN U2007201700393U CN 200720170039 U CN200720170039 U CN 200720170039U CN 201075087 Y CN201075087 Y CN 201075087Y
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- mercury
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- atomizer
- steam generator
- photoinduction
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Abstract
The utility model provides an Hg element morphological analyser used in the analytical chemistry field. The Hg element morpha analysing device comprises a sample introduction part, a medium selection entering control part, a photoinduced steam generator, a gas/liquid separator and a detector. The sample introduction part and the medium selection entering control part are connected with one end of the photoinduced steam generator; the other end of the photoinduced steam generator is connected with the gas/liquid separator; the gas is input into the detector 11 for detection after passing through the gas/liquid separator. The utility model has the advantages of leading the different morpha of the Hg element to selectively occur by adopting a sequence injection-photoinduction-selective Hg steam generation sample introduction system, implementing effective separation of different Hg morpha; increasing the fluorescence detection area, shortening the distance between the detector and an atomizer, and improving detection sensitiveness by adopting the integration design of the atomizer (absorbing pool), fluorescence excitation and fluorescence detection to detector design.
Description
Technical field
The utility model belongs to light, mechanical, electrical integrated analysis instrument, be the mercury element morphological analysis instrument that uses in a kind of analytical chemistry field, especially relate to the device that instrument can be measured simultaneously to the different shape of mercury in institute's specimen under not by means of the situation of any pre-separation technology.
Background technology
Mercury is as a kind of hypertoxicity element, and its toxicity and its occurrence status in sample is closely related, and for example methyl mercury is more a lot of greatly than inorganic mercury toxicity.At present; all very pay close attention to the morphological analysis of mercury both at home and abroad; the sample that relates to fields such as food security, environmental protection not only will carry out the mensuration of total mercury; also to measure, for example require total mercury in the food and organic mercury are measured (GB/T 5009.17-2003) in the state food examination criteria of China's promulgation in 2003 form of mercury.But morphological analysis is mainly some coupling techniques about mercury element both at home and abroad at present, and these technology at first make the different shape pre-separation of mercury with isolation technics commonly used, use atomic spectrum (mass spectrum) to measure as testing tool then.Mainly comprise: high performance liquid chromatography-plasma mass coupling (HPLC-ICP-MS), high performance liquid chromatography-atomic absorption coupling (HPLC-AAS), high performance liquid chromatography-atomic fluorescence coupling (HPLC-AFS) and gas chromatography combined with mass spectrometry (GC-MS).These coupling techniques exist apparatus expensive, the high deficiency of operating cost.Particularly the general requirement of HPLC and GC technology sampling amount is very little, usually in micro updating (μ L) level, and ICP-MS, FAAS, AFS need milliliter level (mL) sample usually, because sampling amount very little causes the detection lower limit deficiency of these coupling techniques, can not satisfy the test request of many actual samples usually like this.
Summary of the invention
In order to overcome the existing mercury morphological analysis technology that is used for, provide a kind of mercury element morphological analysis means in the deficiency aspect equipment/operating cost and the detection lower limit.
The technical scheme that its technical matters that solves the utility model adopts is:
A kind of mercury element morphological analysis means comprises that sample introduction parts 2, medium selection enter control assembly, photoinduction steam generator 6, gas-liquid separator 9 and detecting device 11; Described sample introduction parts 2 are selected to enter control assembly with medium and are connected with described photoinduction steam generator 6 one ends, and the other end of described photoinduction steam generator 6 is connected with gas-liquid separator 9, detects through the gas input detector 11 behind the gas-liquid separator 9.
In concrete application, described medium is selected to enter control assembly and is comprised three solution inlet port and a four-way valve 1; Described four-way valve 1 described three solution inlet port of control and a liquid outlet are selected into/fluid; Described three solution inlet port comprise acetate import, formic acid import and cleaning fluid mouth.
In concrete application, described sample introduction parts 2 are selected to enter control assembly with medium and are connected with photoinduction steam generator 6 with first threeway 5 by peristaltic pump 4, promptly by peristaltic pump 4 and first threeway 5 sample and medium solution are delivered in the photoinduction steam generator 6;
In the middle of described photoinduction steam generator 6 and described gas-liquid separator 9, also comprise second threeway 7, and inject argon gas by an inlet 8 of described second threeway 7; The mercuryvapour that promptly passes through described photoinduction steam generator 6 and produce and the argon gas of injection together enter gas-liquid separator 9 and carry out gas-liquid separation;
In the middle of described gas-liquid separator 9 and detecting device 11, also comprise a mercury enrichment pipe 10; Promptly carry out the gas enrichment through the mercury vapour input mercury enrichment pipe 10 after separating.
In concrete application, described detecting device 11 is taked atomizer 115, fluorescence excitation 113 and fluoroscopic examination 116 integrated apparatus; Comprise detection system shell 111, detection system inner casing 112, fluorescence excitation 113, entrance slit 114, atomizer 115, fluoroscopic examination 116, mercury vapour inlet 117 and mercury vapour outlet 118.
Described fluorescence excitation 113 is the pen type mercury lamp, and described fluoroscopic examination 116 is a photomultiplier, and described atomizer 115 is an absorption cell; And atomizer 115 adopts the thin flat structure, adopts the quartzy material of hollow; Distance between described pen type mercury lamp 113 and the atomizer 115 is 1-10cm, and the distance between described atomizer 115 and the photomultiplier 116 is 1-10cm.
Distance between preferential described pen type mercury lamp (113) and the atomizer (115) is 2cm, and the distance between described atomizer (115) and the photomultiplier (116) is 1cm.
The technical scheme that the utility model technical solution problem is adopted is to utilize in the formic acid medium, and the mercury of different shapes such as inorganic mercury ion, organic mercury can be at the UV light-induced mercury vapour that generates down; And in acetic acid medium, have only organic mercury can be induced the generation mercury vapour, so the selective chemical steam that can reach different shape mercury by the change reaction medium takes place.The cold steam that produces is by after the enrichment of one-level amalgam, and the heating of the mercury vapour of enrichment discharges into detection system, detects with the principle of atomic fluorescence.
The beneficial effects of the utility model are: (1) adopts sequential injection-photoinduction-selectivity mercury vapour generation sampling system, and the different shape selectivity of mercury element is taken place, and has realized effective separation of different shape mercury; (2) detector design is taked atomizer (absorption cell), fluorescence excitation, fluoroscopic examination integrated design, has increased the fluoroscopic examination area, has shortened the distance between detecting device and the atomizer, has improved mensuration sensitivity.
And the instrumentation that the utility model is developed need be by means of pre-separation technology such as HPLC and GC, reaches selective determination to the mercury different shape according to mercury selective chemical steam in the differential responses medium of different shape.But because large volume sampling (2-10ml), and taked incorporate detection system, made this special use instrument can finish mensuration in proper order, measured lower limit and can reach pieck stage (pg) level, low 2-3 the order of magnitude of conventional at present coupling technique different shape mercury.
Description of drawings
Fig. 1 is the principle schematic of the utility model mercury element morphological analysis means;
Fig. 2 is the integrated detecting device in the utility model mercury element morphological analysis means;
Fig. 3 carries out sequential injection selectivity mercury vapour generation sampling system synoptic diagram in the analytical approach for the utility model utilizes the mercury element morphological analysis means.
More than each width of cloth accompanying drawing will specifically describe in detail in conjunction with following embodiment.
Embodiment
Fig. 1 is the principle schematic of the utility model mercury element morphological analysis means.
A kind of mercury element morphological analysis means shown in Figure 1 comprises that sample introduction parts 2, medium selection enter control assembly, photoinduction steam generator 6, gas-liquid separator 9 and detecting device 11; Described sample introduction parts 2 are selected to enter control assembly with medium and are connected with described photoinduction steam generator 6 one ends, and the other end of described photoinduction steam generator 6 is connected with gas-liquid separator 9, detects through the gas input detector 11 behind the gas-liquid separator 9.3 is waste liquid outlet
Described medium is selected to enter control assembly and is comprised three solution inlet port and a four-way valve 1; Described four-way valve 1 described three solution inlet port of control and a liquid outlet are selected into/fluid (concrete selection course please refer to Fig. 3); Described three solution inlet port comprise acetate import, formic acid import and cleaning fluid mouth.
Described sample introduction parts 2 are selected to enter control assembly with medium and are connected with photoinduction steam generator 6 with first threeway 5 by peristaltic pump 4, promptly by peristaltic pump 4 and first threeway 5 sample and medium solution are delivered in the photoinduction steam generator 6;
In the middle of described photoinduction steam generator 6 and described gas-liquid separator 9, also comprise second threeway 7, and inject argon gas by an inlet 8 of described second threeway 7; The mercuryvapour that promptly passes through described photoinduction steam generator 6 and produce and the argon gas of injection together enter gas-liquid separator 9 and carry out gas-liquid separation;
In the middle of described gas-liquid separator 9 and detecting device 11, also comprise a mercury enrichment pipe 10; Promptly carry out the gas enrichment through the mercury vapour input mercury enrichment pipe 10 after separating.
Described detecting device 11 is taked atomizer 115, fluorescence excitation 113 and fluoroscopic examination 116 integrated apparatus; Detecting device 11 comprises detection system shell 111, detection system inner casing 112, fluorescence excitation 113, entrance slit 114, atomizer 115, fluoroscopic examination 116, mercury vapour inlet 117 and mercury vapour outlet 118.
Described fluorescence excitation 113 is the pen type mercury lamp, and described fluoroscopic examination 116 is a photomultiplier, and described atomizer 115 is an absorption cell; And atomizer 115 adopts the thin flat structure, adopts the quartzy material of hollow; Distance between described pen type mercury lamp 113 and the atomizer 115 is 1-10cm, and the distance between described atomizer 115 and the photomultiplier 116 is 1-10cm.
Distance between described pen type mercury lamp (113) and the atomizer (115) is 2cm, and the distance between described atomizer (115) and the photomultiplier (116) is 1cm.
Fig. 2 is the integrated detecting device in the utility model mercury element morphological analysis means
Described detecting device 11 is taked atomizer 115, fluorescence excitation 113 and fluoroscopic examination 116 integrated apparatus; Detecting device 11 comprises detection system shell 111, detection system inner casing 112, fluorescence excitation 113, entrance slit 114, atomizer 115, fluoroscopic examination 116, mercury vapour inlet 117 and mercury vapour outlet 118.
Described fluorescence excitation 113 is the pen type mercury lamp, and described fluoroscopic examination 116 is a photomultiplier, and described atomizer 115 is an absorption cell; And the distance between described pen type mercury lamp 113 and the atomizer 115 is 1-10cm, and the distance between described atomizer 115 and the photomultiplier 116 is 1-10cm.
Wherein, pen type mercury lamp 113 sends the radiant light with specific wavelength and enters atomizer 115 by entrance slit 114, mercury atom in the excited atom device 115 (absorption cell) makes it transit to high-energy state, the mercury atom of high-energy state gives off its feature when getting back to ground state or low-energy state fluorescent line carries out measuring after the opto-electronic conversion after being accepted by photomultiplier 116.Carried out the integrated design of atomizer 115, fluoroscopic examination 116 and fluorescence excitation 113 in the present invention.Distance between fluorescence excitation 113 and the atomizer 115 is 2cm, and the distance between atomizer 115 and the fluoroscopic examination 116 is 1cm.Ultrashort light path has reduced the loss of light, helps to improve the sensitivity of mensuration.In addition, atomizer 115 adopts ultra-thin dull and stereotyped hollow quartz material to make, and helps the area of detection that concentrates and increase fluorescence in the mercury element part, helps to improve the sensitivity of mensuration.
Fig. 3 carries out sequential injection selectivity mercury vapour generation sampling system synoptic diagram in the analytical approach for the utility model utilizes the mercury element morphological analysis means.
A kind of method of utilizing the mercury element morphological analysis means to carry out the mercury element morphological analysis
Described method comprises:
Fig. 3 (A) formic acid medium analysis step: operation four-way valve 1 rotates, and o, a position are communicated, and pumps into formic acid, and pumps into sample from sample pipe 2; Described sample and formic acid converge and enter described photoinduction steam generator 6 in first threeway 5, this moment comprises organic in the test solution and total mercury solution inorganic mercury can produce mercury vapour under UV light-induced, after described gas-liquid separator 9 separated, described mercury vapour was brought into described enrichment pipe 10 by argon gas;
Fig. 3 (B) cleans and testing procedure a: operation four-way valve 1 rotates, and o, b position are communicated, and pumps into the water pipe blow-through, will be captured in the mercury release on the enrichment pipe 10 simultaneously after, enter described detecting device 11 and detect, record the content of total mercury;
Fig. 3 (C) acetic acid medium analytical procedure: operation four-way valve 1 rotates, and o, c position are communicated, and pumps into acetate, and pumps into sample from sample pipe 2; Sample and acetate converge and enter described photoinduction steam generator 6 in first threeway 5, organic mercury optionally produces mercury vapour in the test solution under UV light-induced at this moment, after described gas-liquid separator 9 separated, described mercury vapour was brought into described enrichment pipe 10 by argon gas;
Fig. 3 (D) cleans and testing procedure b: operation four-way valve 1 rotates, and o, b position are communicated, and pumps into the water pipe blow-through, will be captured in the mercury release on the enrichment pipe 10 simultaneously after, enter described detecting device 11 and detect, record organomercurial content.
1 is four-way valve among the figure, a-formic acid inlet, b-filter washing water inlet, c-acetate inlet, o-outlet; The 2nd, sample inlet; The 4th, peristaltic pump; The 5th, first threeway; The 6th, the photoinduction steam generator.
The concentration of described formic acid medium solution is: 0.05-40% (V/V)
The concentration of described acetic acid medium solution is: 0.05-20% (V/V)
Carry out ultraviolet at described photoinduction steam generator and produce in the process of mercury vapour, the time of ultraviolet irradiation is: 5-1200s.
Claims (6)
1. a mercury element morphological analysis means is characterized in that: comprise that sample introduction parts (2), medium selection enter control assembly, photoinduction steam generator (6), gas-liquid separator (9) and detecting device (11); Described sample introduction parts (2) are selected to enter control assembly with medium and are connected with described photoinduction steam generator (6) one ends, the other end of described photoinduction steam generator (6) is connected with gas-liquid separator (9), detects through the gas input detector (11) behind the gas-liquid separator (9).
2. a kind of mercury element morphological analysis means according to claim 1 is characterized in that: described medium is selected to enter control assembly and is comprised three solution inlet port and a four-way valve (1); Described four-way valve (1) described three solution inlet port of control and a liquid outlet; Described three solution inlet port comprise acetate import, formic acid import and cleaning fluid mouth.
3. a kind of mercury element morphological analysis means according to claim 1, it is characterized in that: described sample introduction parts are selected to enter control assembly with medium and are connected with photoinduction steam generator (6) with first threeway (5) by peristaltic pump (4), promptly by peristaltic pump (4) and first threeway (5) sample and medium solution are delivered in the photoinduction steam generator (6);
In the middle of described photoinduction steam generator (6) and described gas-liquid separator (9), also comprise second threeway (7), and inject argon gas by an inlet (8) of described second threeway (7); The mercuryvapour that promptly passes through described photoinduction steam generator (6) and produce and the argon gas of injection together enter gas-liquid separator (9) and carry out gas-liquid separation;
In the middle of described gas-liquid separator (9) and detecting device (11), also comprise a mercury enrichment pipe (10); Promptly carry out the gas enrichment through the mercury vapour input mercury enrichment pipe (10) after separating.
4. a kind of mercury element morphological analysis means according to claim 1 is characterized in that: described detecting device (11) is taked atomizer (115), fluorescence excitation (113) and fluoroscopic examination (116) integrated apparatus; Comprise detection system shell (111), detection system inner casing (112), fluorescence excitation (113), entrance slit (114), atomizer (115), fluoroscopic examination (116), mercury vapour inlet (117) and mercury vapour outlet (118).
5. a kind of mercury element morphological analysis means according to claim 4 is characterized in that: described fluorescence excitation (113) is the pen type mercury lamp, and described fluoroscopic examination (116) is a photomultiplier, and described atomizer (115) is an absorption cell; And atomizer (115) adopts the thin flat structure, adopts the quartzy material of hollow; Distance between described pen type mercury lamp (113) and the atomizer (115) is 1-10cm, and the distance between described atomizer (115) and the photomultiplier (116) is 1-10cm.
6. a kind of mercury element morphological analysis means according to claim 5 is characterized in that: the distance between described pen type mercury lamp (113) and the atomizer (115) is 2cm, and the distance between described atomizer (115) and the photomultiplier (116) is 1cm.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNU2007201700393U CN201075087Y (en) | 2007-08-03 | 2007-08-03 | Device for analyzing quicksilver element form |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNU2007201700393U CN201075087Y (en) | 2007-08-03 | 2007-08-03 | Device for analyzing quicksilver element form |
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| CN201075087Y true CN201075087Y (en) | 2008-06-18 |
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| CNU2007201700393U Expired - Lifetime CN201075087Y (en) | 2007-08-03 | 2007-08-03 | Device for analyzing quicksilver element form |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101358924B (en) * | 2007-08-03 | 2011-05-04 | 北京路捷仪器有限公司 | Morphological analysis apparatus for mercury element and analysis method thereof |
| CN103453179A (en) * | 2008-12-10 | 2013-12-18 | 全技术联合公司 | Automated sample injection apparatus, multiport valve, and methods of making and using the same |
| CN105466740A (en) * | 2014-09-29 | 2016-04-06 | 东亚Dkk株式会社 | Mercury automatic detection system and preprocessing device thereof |
-
2007
- 2007-08-03 CN CNU2007201700393U patent/CN201075087Y/en not_active Expired - Lifetime
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101358924B (en) * | 2007-08-03 | 2011-05-04 | 北京路捷仪器有限公司 | Morphological analysis apparatus for mercury element and analysis method thereof |
| CN103453179A (en) * | 2008-12-10 | 2013-12-18 | 全技术联合公司 | Automated sample injection apparatus, multiport valve, and methods of making and using the same |
| CN105466740A (en) * | 2014-09-29 | 2016-04-06 | 东亚Dkk株式会社 | Mercury automatic detection system and preprocessing device thereof |
| CN105466740B (en) * | 2014-09-29 | 2020-01-03 | 东亚Dkk株式会社 | Mercury automatic detection system and preprocessing device thereof |
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Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| C56 | Change in the name or address of the patentee |
Owner name: BEIJING RUIGUANG INSTRUMENT CO., LTD. Free format text: FORMER NAME: BEIJING LWL INSTRUMENT CO., LTD. |
|
| CP03 | Change of name, title or address |
Address after: 100015, M5 building, 5 floors, workshop of Seven Star Huadian Industrial Park, No. 1, Jiuxianqiao East Road, Beijing, Chaoyang District Patentee after: Beijing Ruiguang Instrument Co., Ltd. Address before: 100016, M5 building, No. 1 East Jiuxianqiao Road, Beijing, Chaoyang District Patentee before: Beijing LWL Instrument Co., Ltd. |
|
| ASS | Succession or assignment of patent right |
Owner name: BEIJING BOHUI INNOVATION TECHNOLOGY CO., LTD. Free format text: FORMER OWNER: BEIJING RUIGUANG INSTRUMENT CO., LTD. Effective date: 20141031 |
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| C41 | Transfer of patent application or patent right or utility model | ||
| COR | Change of bibliographic data |
Free format text: CORRECT: ADDRESS; FROM: 100015 CHAOYANG, BEIJING TO: 102206 CHANGPING, BEIJING |
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| TR01 | Transfer of patent right |
Effective date of registration: 20141031 Address after: 102206 No. 9 middle road, Changping District life science and Technology Park, Beijing Patentee after: Beijing Bohui Innovation Technology Co., Ltd. Address before: 100015, M5 building, 5 floors, workshop of Seven Star Huadian Industrial Park, No. 1, Jiuxianqiao East Road, Beijing, Chaoyang District Patentee before: Beijing Ruiguang Instrument Co., Ltd. |
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| CX01 | Expiry of patent term |
Granted publication date: 20080618 |
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| CX01 | Expiry of patent term |